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Method for synthesis of nanometer ZSM-5 molecular sieve from mother liquor flocculate

A technology of ZSM-5 and molecular sieve, which is applied in the direction of nanotechnology, nanotechnology, nanotechnology, etc. for materials and surface science, can solve the problems of high water content and low content of effective components, and reduce the cost of raw materials and improve Nucleation rate, effect of reducing nucleation activation energy

Inactive Publication Date: 2016-10-26
JIANGSU TIANNUO NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the low content of effective components and high water content in the mother liquor, the direct use of the mother liquor to synthesize molecular sieves has certain limitations.

Method used

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  • Method for synthesis of nanometer ZSM-5 molecular sieve from mother liquor flocculate
  • Method for synthesis of nanometer ZSM-5 molecular sieve from mother liquor flocculate
  • Method for synthesis of nanometer ZSM-5 molecular sieve from mother liquor flocculate

Examples

Experimental program
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Effect test

Embodiment 1

[0045] The mother liquor separated after the crystallization in Comparative Example 1 is flocculated to obtain mother liquor floc 50.2g (silicon dioxide: 37.5%; Sodium oxide: 16%) mixed with 130.2g water, add 0.44g sodium hydroxide, stir until Completely dissolve, add 1.1g of sodium metaaluminate into the above solution and stir until completely dissolved. Slowly add 130g of silica sol dropwise to the above mixed solution under stirring conditions to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, the added tetrapropylammonium hydroxide and silicon aluminum The mass ratio of silicon dioxide in the hydrochloride gel is 0.25. Dissolve the above tetrapropylammonium hydroxide in 30.8g of deionized water and stir until completely dissolved to obtain a mixed solution B. Slowly add solution B to A under stirring conditions Make the mixture uniform in the gel, and finally transfer the mixture into a polytetrafluoroethylene-lined stainless steel cry...

Embodiment 2

[0049] The separated mother liquor flocculation after the crystallization in comparative example 2 obtains mother liquor floc 51.4g (silicon dioxide: 40%; Sodium oxide: 14.6%) mixes with 130.2g water, adds 0.9g sodium hydroxide, stirs to Completely dissolve, add 1.2g of sodium metaaluminate into the above solution and stir until completely dissolved. Slowly add 125g of silica sol dropwise to the above mixed solution under stirring conditions to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, the added tetrapropylammonium hydroxide and silicon aluminum The mass ratio of silicon dioxide in the hydrochloride gel is 0.25. Dissolve the above tetrapropylammonium hydroxide in 30.8g of deionized water and stir until completely dissolved to obtain a mixed solution B. Slowly add solution B to A under stirring conditions Make the mixture uniform in the gel, and finally transfer the mixture into a polytetrafluoroethylene-lined stainless steel crystalli...

Embodiment 3

[0053] The mother liquor separated after the crystallization in Comparative Example 3 was flocculated to obtain mother liquor floc 52.3g (silicon dioxide: 40%; sodium oxide: 13.9%) mixed with 130.2g water, adding 1.1g sodium hydroxide, stirring until Completely dissolve, add 1.2g of sodium metaaluminate into the above solution and stir until completely dissolved. Slowly add 120g of silica sol dropwise to the above mixed solution under stirring conditions to form aluminosilicate gel A; weigh a certain amount of tetrapropylammonium hydroxide, and the added tetrapropylammonium hydroxide and silicon aluminum The mass ratio of silicon dioxide in the hydrochloride gel is 0.25. Dissolve the above tetrapropylammonium hydroxide in 30.8g of deionized water and stir until completely dissolved to obtain a mixed solution B. Slowly add solution B to A under stirring conditions Make the mixture uniform in the gel, and finally transfer the mixture into a polytetrafluoroethylene-lined stainles...

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Abstract

The invention relates to a method for synthesis of a nanometer ZSM-5 molecular sieve from mother liquor flocculate and belongs to the field of chemical engineering. The method comprises carrying out flocculation on a ZSM-5 molecular sieve crystallization mother liquor, separating the flocculate, drying the flocculate and recycling the flocculate as a ZSM-5 molecular sieve synthesis raw material. The method flocculates unreacted effective ingredients in the ZSM-5 molecular sieve crystallization mother liquor, recycles the flocculate, prevents synthesis waste liquid discharge, reduces environment pollution, recovers and recycles the mother liquor, saves raw materials and reduces a molecular sieve synthesis cost. Microcrystallines are formed in the mother liquor flocculate after the reaction so that a nucleation rate and quantity of crystal nucleuses in an induction period of crystallization are greatly improved, molecular sieve nucleation activation energy is reduced, crystallization time is shortened, the molecular sieve crystal grain size is reduced and a molecular sieve crystallization degree is improved.

Description

technical field [0001] The invention relates to a method for synthesizing molecular sieves in the field of chemical industry, in particular to a method for synthesizing nanometer ZSM-5 molecular sieves by using mother liquor flocs. Background technique [0002] Zeolite molecular sieve is an important catalyst active component or catalyst carrier in petroleum and chemical industry. After Mobil Petroleum Company of the United States announced the invention of ZSM-5 zeolite molecular sieve in USP3702886 in 1972, due to its high silicon-aluminum ratio, unique three-dimensional cross-channel structure, excellent hydrothermal stability and anti-coking deactivation performance , ZSM-5 molecular sieve has always been the material of choice for fixed bed MTP process catalysts. [0003] Since the distribution of MTP reaction products is greatly affected by diffusion limitation, the modification of ZSM-5 boils down to the optimization of the catalyst in terms of improving the diffusio...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B39/40B82Y30/00
CPCC01B39/40B82Y30/00C01P2002/72C01P2004/03
Inventor 宋洁胡思余倩邢法猛张正怀郭兆民窦涛潘亚军
Owner JIANGSU TIANNUO NEW MATERIAL TECH
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